CN103760123A - Analytical measurement method for didecyl dimethyl ammonium chloride in seawater - Google Patents
Analytical measurement method for didecyl dimethyl ammonium chloride in seawater Download PDFInfo
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- CN103760123A CN103760123A CN201410009543.XA CN201410009543A CN103760123A CN 103760123 A CN103760123 A CN 103760123A CN 201410009543 A CN201410009543 A CN 201410009543A CN 103760123 A CN103760123 A CN 103760123A
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Abstract
The invention discloses an analytical measurement method for didecyl dimethyl ammonium chloride in seawater. The method comprises the following steps of (1) preparing a standard solution of didecyl dimethyl ammonium chloride, charging gradient volumes of standard solution into separating funnels, adding the seawater, a sodium thiosulfate aqueous solution and a color-developing agent solution into each funnel, controlling the pH, and performing shaking uniformizing and complete standing; (2) adding an organic extracting agent into each separating funnel for extraction; (3) extracting an organic layer solution, measuring a light absorption value of the organic layer solution, performing zero adjustment by using the organic extracting agent, and drawing a standard curve by using the organic layer solution as a blank reference solution; (4) measuring the seawater to be measured into the separating funnels, adding the sodium thiosulfate aqueous solution and the color-developing agent solution into the separating funnels, controlling the pH, and performing shaking uniformizing and complete standing; (5) adding the organic extracting agent into each separating funnel for extraction; and (6) extracting an organic layer solution, measuring a light absorption value of the organic layer solution, and calculating the concentration of the didecyl dimethyl ammonium chloride in the seawater according to the standard curve. The method is accurate, reliable and easy to operate.
Description
Technical field
The present invention relates to the analysis determining method of DDAC in a kind of seawater.
Background technology
DDAC is a kind of cationic surfactant, and DDAC is one of third generation product of quaternary ammonium salt bactericide, and it has the stronger ability of killing to microorganism, can be used for oil-field flooding and industrial cooling circulating water system and makes germifuge and Biocidal algae-killing agent etc.The mechanism of action of this series bactericidal agent is mainly that kation passes through the effects such as hydrophobic binding between electrostatic force, hydrogen bond force and surfactant molecule and protein molecule, adsorb electronegative bacterial body, be gathered on cell membrane, generating chamber's inhibition effect, causes bacterial growth suppressed and dead; Simultaneously its hydrophobic alkyl can also with the hydrophilic group effect of microorganism, change the permeability of film, then there is lysis, destroy eucaryotic cell structure, cause dissolving and the death of cell.The in line cooling water system process field of seawater is applied to kill the microorganisms such as shellfish in Cooling system pipe, and dosage is at 1ppm.Although DDAC belongs to lower toxicity germifuge, Drug level is low, but still needs strict its concentration of emission of controlling.
For the content analysis of such short carbon chain quaternary ammonium salt, mainly contain chemical method and instrumental method, international standard and China standard GB/T5174 all adopt chemical titration analysis, but chemical method detection limit is higher, are not suitable for this type of trace detection.And more employing ultraviolet spectrophotometer is analyzed it in instrumental method, in existing published method, nearly all under this single environment of pure water, by extraction chloroform layer, undertaken and spectral analysis.There is scholar at disclosed < < in 2004 in the Central-South pharmacy > > second phase, in " content of Wan withAcid-dye Colorimetry low concentration benzalkonium bromide solution " literary composition, utilize benzalkonium bromide to form stabilizing ion with bromophenol blue under alkali condition and there is good uv absorption, and easily by the character of chloroform extraction, recorded its content.But this method is not also suitable for the microanalysis of the quaternary ammonium salt in complex dielectrics as this in seawater.Experiment shows that from seawater the light absorption value that chloroform layer that extraction obtains obtains when carrying out ultra-violet analysis is extremely unstable, even decays to zero.Within 2010, at < < physical and chemical inspection-chemical fascicle > >, in the second phase, there is one piece of article of publishing " content of quaternary ammonium salt in determined by ultraviolet spectrophotometry seawater ", but in article, do not mention analyzed quaternary ammonium salt type, and itself have uv absorption without adding developer, and in the present invention DDAC itself without uv absorption, need analyze again by processing, so situation is more complicated during the content of this medicament using in analyzing seawater.
Summary of the invention
The object of the present invention is to provide the analysis determining method of DDAC in a kind of seawater.
The technical solution used in the present invention is:
An analysis determining method for DDAC in seawater, comprises the following steps:
1) standard solution of the DDAC that compound concentration is 10-20ppm, get standard solution that some parts of volumes change in gradient in separating funnel, to all adding three kinds of materials in each separating funnel: seawater, sodium thiosulfate solution, chromogenic reagent solution, the pH that controls solution is 2≤pH < 7, shakes up and sufficient standing;
2) in each separating funnel, add organic extractant, fully shake separating funnel and fully extract, static layering;
3) get organic layer solution, at 410-490 nm place, with ultraviolet spectrophotometer, measure its light absorption value A, and return to zero with organic extractant, and as blank reference liquid, drawing standard curve;
4) measure some parts of seawater to be measured and add in separating funnel, then add sodium thiosulfate solution, chromogenic reagent solution in separating funnel, the pH that controls solution is 2≤pH < 7, shakes up and sufficient standing;
5) in each separating funnel, add organic extractant, fully shake separating funnel and fully extract, static layering;
6) get organic layer solution, with ultraviolet spectrophotometer, measuring its light absorption value with the same wavelength of step 3) place, according to the typical curve of gained, calculate DDAC concentration in seawater.
In step 1) and step 4), the concentration of sodium thiosulfate solution is 0.1-1mol/L.
In step 1), in the standard solution that described volume changes in gradient, minimum volume is 0.5-1.5ml, and maximum volume is 7.5-10.5ml.
In step 1), in each separating funnel, the addition of seawater is 8-12mL.
In step 1), utilize weak acid to control the pH of solution, described weak acid comprises carbonic acid, acetic acid, oxalic acid, sulphurous acid.
In step 1), the solvent of the standard solution of DDAC is seawater.
In step 1) and step 4), the mass concentration of chromogenic reagent solution is 0.1-0.2wt%; Described developer is at least one in acid blue, thymol blue, orange II, alizarin yellow R, methyl orange.
In step 1), the sodium thiosulfate in sodium thiosulfate solution, the developer in chromogenic reagent solution, seawater three's addition ratio is: 0.02-0.2mmol:(2-4) * 10
-4mg:10ml; In step 4), the sodium thiosulfate in sodium thiosulfate solution, the developer in chromogenic reagent solution, seawater three's addition ratio is: 0.02-0.2mmol:(2-4) * 10
-4mg:10ml.
Step 2), in, the addition of organic extractant is 8-12mL; Described organic extractant is at least one in methylene chloride, ethylene dichloride, propylene dichloride, methenyl choloride, bromochloromethane, methylene bromide, bromochloroethane, ethylene dibromide, ether.
At least one in step 5) in organic extractant methylene chloride used, ethylene dichloride, propylene dichloride, methenyl choloride, bromochloromethane, methylene bromide, bromochloroethane, ethylene dibromide, ether.
The invention has the beneficial effects as follows: method of testing of the present invention is accurately reliable, simple to operation.Specifically:
In Seawater, composition is extremely complicated, there is the factor of much analytical test being disturbed, analysis test method of the present invention can be compared with the concentration of the DDAC in this complex dielectrics of Accurate Measurement seawater, quick and precisely simple to operation, parallel testing several times, the relative deviation of the data obtained is little.
Accompanying drawing explanation
Fig. 1 is the typical curve of embodiment 1 gained.
Embodiment
An analysis determining method for DDAC in seawater, comprises the following steps:
1) standard solution of the DDAC that compound concentration is 10-20ppm, get standard solution that some parts of volumes change in gradient in separating funnel, to all adding three kinds of materials in each separating funnel: seawater, sodium thiosulfate solution, developer aqueous solution, the pH that controls solution is 2≤pH < 7, shakes up and sufficient standing;
2) in each separating funnel, add organic extractant, fully shake separating funnel and fully extract, static layering;
3) get organic layer solution, at 410-490 nm place, with ultraviolet spectrophotometer, measure its light absorption value A, and return to zero with organic extractant, and as blank reference liquid, drawing standard curve;
4) measure some parts of seawater to be measured and add in separating funnel, then add sodium thiosulfate solution, developer aqueous solution in separating funnel, the pH that controls solution is 2≤pH < 7, shakes up and sufficient standing;
5) in each separating funnel, add organic extractant, fully shake separating funnel and fully extract, static layering;
6) get organic layer solution, with ultraviolet spectrophotometer, measuring its light absorption value with the same wavelength of step 3) place, according to the typical curve of gained, calculate DDAC concentration in seawater.
In step 1) and step 4), the concentration of sodium thiosulfate solution is 0.1-1mol/L.
In step 1), in the standard solution that described volume changes in gradient, minimum volume is 0.5-1.5ml, and maximum volume is 7.5-10.5ml.
In step 1), in each separating funnel, the addition of seawater is 8-12mL.
In step 1), utilize weak acid to control the pH of solution, described weak acid comprises carbonic acid, acetic acid, oxalic acid, sulphurous acid.
In step 1) and step 4), the mass concentration of developer aqueous solution is 0.1-0.2wt%; Described developer is at least one in acid blue, thymol blue, orange II, alizarin yellow R, methyl orange.
In step 1), the developer in the sodium thiosulfate in sodium thiosulfate solution, developer aqueous solution, seawater three's addition ratio is: 0.02-0.2mmol:(2-4) * 10
-4mg:10ml; In step 4), the developer in the sodium thiosulfate in sodium thiosulfate solution, developer aqueous solution, seawater three's addition ratio is: 0.02-0.2mmol:(2-4) * 10
-4mg:10ml.
Step 2), in, the addition of organic extractant is 8-12mL; Described organic extractant is at least one in methylene chloride, ethylene dichloride, propylene dichloride, methenyl choloride, bromochloromethane, methylene bromide, bromochloroethane, ethylene dibromide, ether.
At least one in step 5) in organic extractant methylene chloride used, ethylene dichloride, propylene dichloride, methenyl choloride, bromochloromethane, methylene bromide, bromochloroethane, ethylene dibromide, ether; Preferably, organic extractant used organic extractant and step 2 used) is identical.
It should be noted that, in the present invention:
In step 1), the standard solution solvent used of preparation DDAC is seawater, and this solvent seawater blank seawater that the seawater to one of three kinds of materials that add in each separating funnel described in step is not containing DDAC therewith (is without dispensing, to process in seawater, take this blank seawater is the standard solution of solvent preparation DDAC, can from solvent, additionally not introduce DDAC).
The seawater of seawater to be measured in step 4) for processing through dispensing,, for the seawater in step 1), has added medicine DDAC wherein;
As described in the background art, the in line cooling water system process field of seawater is applied to kill the microorganisms such as shellfish in Cooling system pipe by its (being DDAC).
Following enumerated embodiment is also such: in drawing standard curve step, related seawater is the blank seawater that does not add medicine;
Therefore,, with the standard solution of this blank seawater preparation DDAC, can from solvent, additionally not bring DDAC into.
And in the step of the preparation and determination methods of sample, the seawater of seawater to be measured for processing through dispensing.
Object of the present invention is also measured the concentration of DDAC in the seawater of processing through dispensing just.
Below in conjunction with specific embodiment, the present invention is described further:
embodiment 1
(1) drawing standard curve: the DDAC standard solution that the seawater of take is 13.36ppm as solvent compound concentration; The aqueous solution of acid blue 80 and the sodium thiosulfate solution of 0.1mol/L that preparation mass concentration is 0.1%.With transfer pipet draw respectively 1,2,4,6, the standard solution of 8ml is in five separating funnels, add respectively 10ml seawater, 0.2mL sodium thiosulfate solution and 0.2mL acid blue, and be 3 with acetic acid control pH value of solution, shake up after rear static placement 30 min, with pipette, extract 10ml ethylene dichloride (reagent is pure), add respectively in five separating funnels, fully shake separating funnel, component to be measured is fully extracted into organic phase, static layering afterwards, obtains that concentration is respectively 1.336,2.672,5.344,8.016, the solution of 10.688ppm; Get respectively in organic phase to 5 cuvette.At 410 nm places, with ultraviolet spectrophotometer, measure its light absorption value, with ethylene dichloride zeroing, and as blank reference liquid, drawing standard curve, is shown in accompanying drawing 1.
(2) preparation and determination methods of sample: accurately measure the Duplicate Samples of 5 part of 200 ml seawater to be measured in 5 separating funnels, add the sodium thiosulfate solution 4mL of 0.1mol/L and the aqueous solution 4mL of the acid blue 80 that mass concentration is 0.1%, with acetic acid, controlling its pH is 3, shakes up.With transfer pipet, add respectively the extraction of 20ml ethylene dichloride again, take off a layer organic phase, under same wave number, (410nm) records 5 groups of light absorption values and is respectively 0.07,0.069,0.069,0.068,0.069, according to typical curve, draw DDAC mean concentration 4.8857 ppm in seawater, calculating its relative standard deviation is 1.14%.
(3) calculating of blank recovery of standard addition: the DDAC solution 1ml that accurately measures 104ppm not in dosing seawater, tests it containing measure 5.3911ppm by step (2) in 200 ml, calculates its blank recovery of standard addition=102.4%
embodiment 2
(1) drawing standard curve: the DDAC standard solution that the seawater of take is 10 ppm as solvent compound concentration; The aqueous solution of methyl orange and the sodium thiosulfate solution of 0.1mol/L that preparation mass concentration is 0.1%.With transfer pipet draw respectively 1,2,4,6, the standard solution of 8ml is in five separating funnels, add respectively 10ml seawater, 0.2mL sodium thiosulfate solution and 0.2mL methyl orange, and be 3 with acetic acid control pH value of solution, shake up after rear static placement 20 min, with pipette, extract 10ml methylene chloride (reagent is pure), add respectively in five separating funnels, fully shake separating funnel, component to be measured is fully extracted into organic phase, static layering afterwards, obtains concentration and is 1,2,4,6, the solution of 8ppm; Get respectively in organic phase to 5 cuvette.At 440 nm places, with ultraviolet spectrophotometer, measure its light absorption value, with methylene chloride zeroing, and as blank reference liquid, typical curve, y=0.0195x+0.0093, R
2=0.9995.
(2) preparation and determination methods of sample: accurately measure 5 part of 200 ml seawater sample to be measured in 5 separating funnels, add the sodium thiosulfate solution 4mL of 0.1mol/L and the aqueous solution 4mL of the methyl orange that mass concentration is 0.1%, controlling its pH with acetic acid is 3, shakes up.With transfer pipet, add respectively 20ml dichloromethane extraction again, take off a layer organic phase, under same wave number, survey its light absorption value and be respectively 0.102,0.105,0.106,0.104,0.105, according to typical curve, calculating DDAC mean concentration in seawater is 4.8769ppm, and to calculate its relative standard deviation be 1.59%.
embodiment 3
(1) drawing standard curve: the DDAC standard solution that the seawater of take is 15 ppm as solvent compound concentration; The aqueous solution of Acid Orange II and the sodium thiosulfate solution of 0.2mol/L that preparation mass concentration is 0.1%.With transfer pipet draw respectively 1,2,4,6, the standard solution of 8ml in five separating funnels, add respectively 10ml seawater, 0.2mL sodium thiosulfate solution and 0.2mL Acid Orange II, and with acetic acid, to control pH value of solution be 5, shake up rear static placement 15 min.Afterwards, with pipette, extract 10ml bromochloromethane (reagent is pure), add respectively in five separating funnels, fully shake separating funnel, component to be measured is fully extracted into organic phase, static layering afterwards, obtains concentration and is 1.5,3,6,9, the solution of 12ppm; Get respectively in organic phase to 5 cuvette.At 484 nm places, with ultraviolet spectrophotometer, measure its light absorption value, with bromochloromethane zeroing, and as blank reference liquid, drawing standard curve y=0.0209x+0.0124, R
2=0.9995.
(2) preparation and determination methods of sample: accurately measure 5 part of 250 ml seawater sample to be measured in 5 separating funnels, add the sodium thiosulfate solution 5mL of 0.1mol/L and the aqueous solution 5mL of the Acid Orange II that mass concentration is 0.1%
,with acetic acid, controlling its pH is 5, shakes up.With transfer pipet, add respectively the extraction of 25ml bromochloromethane again, take off a layer organic phase, under same wave number, survey its light absorption value and be respectively 0.113,0.113,0.112,0.115,0.113, according to typical curve, calculating DDAC mean concentration in seawater is 4.8230ppm, and to calculate its relative standard deviation be 1.09%.
Claims (10)
1. an analysis determining method for DDAC in seawater, is characterized in that: comprise the following steps:
1) standard solution of the DDAC that compound concentration is 10-20ppm, get standard solution that some parts of volumes change in gradient in separating funnel, to all adding three kinds of materials in each separating funnel: seawater, sodium thiosulfate solution, chromogenic reagent solution, the pH that controls solution is 2≤pH < 7, shakes up and sufficient standing;
2) in each separating funnel, add organic extractant, fully shake separating funnel and fully extract, static layering;
3) get organic layer solution, at 410-490 nm place, with ultraviolet spectrophotometer, measure its light absorption value A, and return to zero with organic extractant, and as blank reference liquid, drawing standard curve;
4) measure some parts of seawater to be measured and add in separating funnel, then add sodium thiosulfate solution, chromogenic reagent solution in separating funnel, the pH that controls solution is 2≤pH < 7, shakes up and sufficient standing;
5) in each separating funnel, add organic extractant, fully shake separating funnel and fully extract, static layering;
6) get organic layer solution, with ultraviolet spectrophotometer, measuring its light absorption value with the same wavelength of step 3) place, according to the typical curve of gained, calculate DDAC concentration in seawater.
2. the analysis determining method of DDAC in a kind of seawater according to claim 1, is characterized in that: in step 1) and step 4), the concentration of sodium thiosulfate solution is 0.1-1mol/L.
3. the analysis determining method of DDAC in a kind of seawater according to claim 1, it is characterized in that: in step 1), in the standard solution that described volume changes in gradient, minimum volume is 0.5-1.5ml, and maximum volume is 7.5-10.5ml.
4. the analysis determining method of DDAC in a kind of seawater according to claim 1, is characterized in that: in step 1), in each separating funnel, the addition of seawater is 8-12mL.
5. the analysis determining method of DDAC in a kind of seawater according to claim 1, is characterized in that: in step 1), utilize weak acid to control the pH of solution, described weak acid comprises carbonic acid, acetic acid, oxalic acid, sulphurous acid.
6. the analysis determining method of DDAC in a kind of seawater according to claim 1, is characterized in that: in step 1), the solvent of the standard solution of DDAC is seawater.
7. the analysis determining method of DDAC in a kind of seawater according to claim 1, is characterized in that: in step 1) and step 4), the mass concentration of chromogenic reagent solution is 0.1-0.2wt%; Described developer is at least one in acid blue, thymol blue, orange II, alizarin yellow R, methyl orange.
8. the analysis determining method of DDAC in a kind of seawater according to claim 1, it is characterized in that: in step 1), the sodium thiosulfate in sodium thiosulfate solution, the developer in chromogenic reagent solution, seawater three's addition ratio is: 0.02-0.2mmol:(2-4) * 10
-4mg:10ml; In step 4), the sodium thiosulfate in sodium thiosulfate solution, the developer in chromogenic reagent solution, seawater three's addition ratio is: 0.02-0.2mmol:(2-4) * 10
-4mg:10ml.
9. the analysis determining method of DDAC in a kind of seawater according to claim 1, is characterized in that: step 2) in, the addition of organic extractant is 8-12mL; Described organic extractant is at least one in methylene chloride, ethylene dichloride, propylene dichloride, methenyl choloride, bromochloromethane, methylene bromide, bromochloroethane, ethylene dibromide, ether.
10. the analysis determining method of DDAC in a kind of seawater according to claim 1, is characterized in that: at least one in step 5) in organic extractant methylene chloride used, ethylene dichloride, propylene dichloride, methenyl choloride, bromochloromethane, methylene bromide, bromochloroethane, ethylene dibromide, ether.
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|---|---|---|---|---|
| CN104458394A (en) * | 2014-12-30 | 2015-03-25 | 江南大学 | Method of improving detection sensitivity of formaldehyde with diacetone spectrophotometry |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458394A (en) * | 2014-12-30 | 2015-03-25 | 江南大学 | Method of improving detection sensitivity of formaldehyde with diacetone spectrophotometry |
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Address after: No. 318, Guangzhou, Guangdong, Tianhe District Patentee after: GUANGDONG RESEARCH INSTITITUTE OF PETROCHEMICAL AND FINE CHEMICAL ENGINEERING Address before: Tianhe District Tangxia Jubei road 510665 Guangzhou City, Guangdong province No. 318 Patentee before: PETROLEUM AND CHEMICAL Research Institute OF GUANGDONG PROVINCE |
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Address after: 510665 Guangzhou, Guangdong, Tianhe District Province Road West, No. 318 Patentee after: Institute of chemical engineering, Guangdong Academy of Sciences Address before: 510665 Guangzhou, Guangdong, Tianhe District Province Road West, No. 318 Patentee before: GUANGDONG RESEARCH INSTITITUTE OF PETROCHEMICAL AND FINE CHEMICAL ENGINEERING |